EP2017000B1 - Mikrofluidische Geräte für verstärkte Verfahren - Google Patents

Mikrofluidische Geräte für verstärkte Verfahren Download PDF

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Publication number
EP2017000B1
EP2017000B1 EP07301225A EP07301225A EP2017000B1 EP 2017000 B1 EP2017000 B1 EP 2017000B1 EP 07301225 A EP07301225 A EP 07301225A EP 07301225 A EP07301225 A EP 07301225A EP 2017000 B1 EP2017000 B1 EP 2017000B1
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EP
European Patent Office
Prior art keywords
passage
volume
walls
microfluidic device
passages
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EP07301225A
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English (en)
French (fr)
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EP2017000A1 (de
Inventor
Elena Lavric
Pierre Woehl
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Corning Inc
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Corning Inc
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First worldwide family litigation filed litigation Critical https://patents.darts-ip.com/?family=38820340&utm_source=google_patent&utm_medium=platform_link&utm_campaign=public_patent_search&patent=EP2017000(B1) "Global patent litigation dataset” by Darts-ip is licensed under a Creative Commons Attribution 4.0 International License.
Application filed by Corning Inc filed Critical Corning Inc
Priority to EP07301225A priority Critical patent/EP2017000B1/de
Priority to TW097126566A priority patent/TWI363656B/zh
Priority to PCT/US2008/008535 priority patent/WO2009009129A1/en
Priority to MX2010000485A priority patent/MX2010000485A/es
Priority to CN2008801070305A priority patent/CN101873890B/zh
Priority to AU2008275602A priority patent/AU2008275602A1/en
Priority to JP2010516065A priority patent/JP2011508657A/ja
Priority to RU2010104674/05A priority patent/RU2010104674A/ru
Priority to US12/171,403 priority patent/US7939033B2/en
Priority to CA2693463A priority patent/CA2693463A1/en
Priority to KR1020107003067A priority patent/KR101666635B1/ko
Priority to BRPI0813700-5A2A priority patent/BRPI0813700A2/pt
Publication of EP2017000A1 publication Critical patent/EP2017000A1/de
Priority to ZA201000944A priority patent/ZA201000944B/xx
Publication of EP2017000B1 publication Critical patent/EP2017000B1/de
Application granted granted Critical
Priority to JP2014056426A priority patent/JP6204235B2/ja
Priority to JP2017166629A priority patent/JP6674933B2/ja
Priority to JP2020039661A priority patent/JP7049381B2/ja
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    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J19/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J19/0093—Microreactors, e.g. miniaturised or microfabricated reactors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/20—Jet mixers, i.e. mixers using high-speed fluid streams
    • B01F25/25—Mixing by jets impinging against collision plates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/432—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction with means for dividing the material flow into separate sub-flows and for repositioning and recombining these sub-flows; Cross-mixing, e.g. conducting the outer layer of the material nearer to the axis of the tube or vice-versa
    • B01F25/4321—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction with means for dividing the material flow into separate sub-flows and for repositioning and recombining these sub-flows; Cross-mixing, e.g. conducting the outer layer of the material nearer to the axis of the tube or vice-versa the subflows consisting of at least two flat layers which are recombined, e.g. using means having restriction or expansion zones
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433—Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F25/00—Flow mixers; Mixers for falling materials, e.g. solid particles
    • B01F25/40—Static mixers
    • B01F25/42—Static mixers in which the mixing is affected by moving the components jointly in changing directions, e.g. in tubes provided with baffles or obstructions
    • B01F25/43—Mixing tubes, e.g. wherein the material is moved in a radial or partly reversed direction
    • B01F25/433—Mixing tubes wherein the shape of the tube influences the mixing, e.g. mixing tubes with varying cross-section or provided with inwardly extending profiles
    • B01F25/4338—Mixers with a succession of converging-diverging cross-sections, i.e. undulating cross-section
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/30—Micromixers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01F—MIXING, e.g. DISSOLVING, EMULSIFYING OR DISPERSING
    • B01F33/00—Other mixers; Mixing plants; Combinations of mixers
    • B01F33/80—Mixing plants; Combinations of mixers
    • B01F33/81—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles
    • B01F33/811—Combinations of similar mixers, e.g. with rotary stirring devices in two or more receptacles in two or more consecutive, i.e. successive, mixing receptacles or being consecutively arranged
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L3/00—Containers or dishes for laboratory use, e.g. laboratory glassware; Droppers
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00783—Laminate assemblies, i.e. the reactor comprising a stack of plates
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00824—Ceramic
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00819—Materials of construction
    • B01J2219/00831—Glass
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00851—Additional features
    • B01J2219/00858—Aspects relating to the size of the reactor
    • B01J2219/0086—Dimensions of the flow channels
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00873—Heat exchange
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
    • B01J2219/00—Chemical, physical or physico-chemical processes in general; Their relevant apparatus
    • B01J2219/00781—Aspects relating to microreactors
    • B01J2219/00889—Mixing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01L—CHEMICAL OR PHYSICAL LABORATORY APPARATUS FOR GENERAL USE
    • B01L2400/00—Moving or stopping fluids
    • B01L2400/08—Regulating or influencing the flow resistance
    • B01L2400/084—Passive control of flow resistance
    • B01L2400/086—Passive control of flow resistance using baffles or other fixed flow obstructions

Definitions

  • Microfluidic devices include fluidic devices over a scale ranging from microns to a few millimeters, that is, devices with fluid channels the smallest dimension of which is in the range of microns to a few millimeters, and preferably in the range of from about 10's of microns to about 1.5 millimeters.
  • microfluidic devices particularly microreaders, can be useful to perform difficult, dangerous, or even otherwise impossible chemical reactions and processes in a safe, efficient, and environmentally-friendly way. Such improved chemical processing is often described as "process intensification.”
  • Process intensification is a relatively new emphasis in chemical engineering which has the potential to transform traditional chemical processing, leading to smaller, safer, and more energy-efficient and environmentally friendly processes.
  • the principal goal of process intensification is to produce highly efficient reaction and processing systems using configurations that simultaneously significantly reduce reactor sizes and maximize mass-and heat-transler efficiencies. Shortening the development time from laboratory to commercial production through the use of methods that permit the researcher to obtain better conversion or selectivity is also one of the priorities of process intensification studies.
  • Process intensification may be particularly advantageous for the fine chemicals and pharmaceutical industries, where production amounts are often smaller than a few metric tons per year, and where lab results in an intensified process may be relatively easily scaled-out in a parallel fashion.
  • Process intensification consists of the development of novel apparatuses and techniques that, relative to those commonly used today are expected to bring very important improvements in manufacturing and processing, substantially decreasing equipment-size to production-capacity ratio, energy consumption and/or waste production, and ultimately resulting in cheaper, sustainable technologies. Or, to put this in a shorter form: any chemical engineering development that leads to a substantially smaller, cleaner, and more energy efficient technology is process intensification.
  • FIG. 1 is a schematic perspective showing a general layered structure of certain type of micro fluidic device.
  • a microfluidic device 10 of the type shown generally comprises at least two volumes 12 and 14 within which is positioned or structured one or more thermal control passages not shown in detail in the figure.
  • the volume 12 is limited in the vertical direction by horizontal walls 16 and 18, while the volume 14 is limited in the vertical direction by horizontal walls 20 and 22.
  • horizontal and vertical are relative terms only and indicative of a general relative orientation only, and do not necessarily indicate perpendicularity, and are also used for convenience to refer to orientations used in the figures, which orientations are used as a matter of convention only and not intended as characteristic of the devices shown.
  • the present invention and the embodiments thereof to be described herein may be used in any desired orientation, and horizontal and vertical walls need generally only be intersecting walls, and need not be perpendicular.
  • a reactant passage 26, partial detail of which is shown in prior art Figure 2 is positioned within the volume 24 between the two central horizontal walls 18 and 20.
  • Figure 2 shows a cross-sectional plan view of the vertical wall structures 28, some of which define the reactant passage 26, at a given cross-sectional level within the volume 24.
  • the reactant passage 26 in Figure 2 is cross-hatched for easy visibility and includes a more narrow, tortuous passage 30 followed by a broader, less tortuous passage 32. Close examination of the narrow, tortuous passage 30 in Figure 2 will show that the tortuous passage 30 is discontinuous in the plane of the figure.
  • the fluidic connections between the discontinuous sections of the tortuous passage shown in the cross section of Figure 1 are provided in a different plane within the volume 24, vertically displaced from plane of the cross-section shown in Figure 2 . resulting in a passage 30 that is serpentine and three-dimensionally tortuous.
  • the device shown in Figures 1 and 2 and related other embodiments are disclosed in more detail, for example, in European Patent No. EP 01 679 115, C. Guermeur et al. (2005 ).
  • the narrow, more tortuous passage 30 serves to mix reactants white an immediately subsequent broader, less tortuous passage 32 follows the passage 30 and serves to provide a volume in which reactions can be completed while in a relatively controlled thermal environment.
  • thermo- and fluid-dynamic performance of such devices Although good performance has been obtained with devices of this type, in many cases even exceeding the state of the art for a given reaction, it has nonetheless become desirous to improve upon the thermo- and fluid-dynamic performance of such devices. In particular, it is desirable that the heat exchange performance of such devices be improved while simultaneously approximately maintaining at the same level or even decreasing the pressure drop caused by the device, white increasing mixing performance and throughput.
  • a microfluidic device includes at least one reactant passage and one or more thermal control passages defined therein, the one or more thermal control passages being positioned and arranged within two volumes each bordered by a wall, the walls being generally planar and parallel to one another, the reactant passage positioned between said generally planar walls and defined by said generally planar walls and walls extending between said generally planar walls, wherein the reactant passage comprises multiple successive chambers, each such chamber including a split of the reactant passage into at least two sub-passages, and a joining of the split passages, and a change of passage direction, of at least one of the sub-passages, of at least 90 degrees, and wherein each of the multiple successive chambers being immediately succeded by another one of said chambers further comprises a gradually narrowing exit which forms a corresponding narrowed entrance of the succeeding chamber, and a splitting and re-directing wall oriented crossways to the immediately upstream passage and positioned immediately downstream of the chamber's entrance, the upstream side of said splitting and re-directing wall
  • Figure 1 (prior art) is a schematic perspective showing a general layered structure of certain prior art microfluidic devices
  • Figure 2 (prior art) is a cross-sectional plan view of vertical wall structures within the volume 24 of Figure 1 :
  • Figure 3 is a cross-sectional plan view of vertical wall structures defining a reaction passage according to an embodiment of the present invention
  • Figure 4 is a graph of overall heat transfer coefficient in watts per meter-squared and Kelvin as a function of flow rate in milliliters per minute, comparing an embodiment of the invention to a prior art device;
  • Figure 5 is a graph of percentage mixing performance of a test reaction in a micromixer device as a function of flow rate in milliliters per minute, comparing an embodiment of the invention to a prior art device;
  • Figure 6 is a graph of pressure drop across a microf1uidic device in millibar, as a function of flow rate in milliliters per minute, comparing an embodiment of the invention to a prior art device (using a glucose solution of 13 centiPoise);
  • Figure 7 is a digital photograph showing preservation of an emulsion of immiscible liquids in testing of an embodiment of a microfluidic device according to the present invention.
  • Figure 8 is a digital photograph showing coalescing of immiscible liquids in testing of a prior art microfluidic device; same experimental conditions than Figure 17;
  • Figure 9 is another digital photograph showing preservation of an emulsion of immiscible liquids in testing of an embodiment of a microfluidic device according to the present invention, but at a higher flow rate than in Figure 7 , with resulting smaller droplets;
  • Figures 10A-10G are cross-sectional plan views of multiple alternative vertical wall structures defining portions of reaction passages according to some alternative embodiments of the present invention.
  • Figure 11 is a cross-sectional plan view of vertical wall structures defining a portion of a reaction passage according to yet another embodiment of the present invention.
  • Figure 12 is a cross-sectional plan view of alternative vertical wall structures defining portions of a reaction passage according to yet another alternative embodiment of the present invention.
  • Figure 13 is a cross-sectional plan view of multiple test reaction passages according to various alternative embodiments of the present invention corresponding generally to those shown in Figure 9 , laid out as part of a single device.
  • Figure 14 is a graph of pressure in bar as a function of time during solids handling testing of an embodiment of a device according to the present invention.
  • Figure 15 is a graph of specific interfacial area (squared-meter per cubic-meter) as a function of gas injection flowrate in milliliters per minute on the x axis for three different water flow rates as tested in an embodiment of the present invention.
  • Figure 3 is a cross-sectional plan view of vertical wall structures 28 within a microfluidic device according to an embodiment of the present invention.
  • Vertical wall structures 28 define a reactant passage 26 that is positioned between two walls 18, 20 as in Figure 1 , which walls 18, 20 themselves form the reactant-passage-facing boundaries of volumes 12 and 14, in which are contained one ore more thermal control passages (not shown).
  • the walls 18, 20 are generally planar and parallel to each other.
  • reactants may be fed into the reactant passage(s) 26 at locations A and B. and flow out of the reactant passage at both locations C.
  • the reactant passage is defined by said horizontal generally planar walls 18, 20, and walls 28, vertical in the orientation of Figure 1 , extending between said generally planar walls 18, 20.
  • the reactant passage 26 comprises multiple successive chambers 34, each such chamber including a split of the reactant passage into at least two sub-passages 36, and a joining 38 of the split passages 36, and a change of passage direction, in at least one of the sub-passages 36, of at least 90 degrees relative to the immediate upstream passage direction.
  • both sub-passages 36 change direction in excess of 90 degrees relative to the immediate upstream passage direction of the reactant passage 26.
  • each of the multiple successive chambers 34 further comprises a gradually narrowing exit 40 which forms a corresponding narrowed entrance 42 of the succeeding chamber.
  • the chambers 34 also include a splitting and re-directing wall 44 oriented crossways to the immediately upstream flow direction and positioned immediately downstream of the chamber's entrance 42.
  • the upstream side of the splitting and re-directing wall 44 has a concave surface 46.
  • the narrowing exit 40 from one chamber 34 to the next is desirably on the order of about 1 mm width.
  • the channel desirably may have a height of about 800 ⁇ m.
  • the chambers 34 desirably have a constant height H, shown in Figure 1 , in a direction generally perpendicular to the walls 18 and 20, which height H generally corresponds to the distance between the walls 18 and 20.
  • the portion of passage 26 having the chambers 34 generally occupies the maximum space possible in the direction of height H, matching the maximum dimension of the volume 24 in the direction of H.
  • the volume of a given lateral size microfluidic device is thus maximized, allowing longer residence times at higher throughput rates and (2) the amount of material and distance between reactant passage 26 and the volumes 12 and 14 in which one or more thermal control fluid passages are contained is minimized, allowing for greater heat transfer.
  • the height H may desirably be on the order of 800 ⁇ m to in excess of a few millimeters, the thickness of boundary layers in the direction of H are generally reduced by secondary flows induced within the reactant passage by passing of the reactant fluid through the directional changes caused by the splitting and re-directing walls 44, and by repeated passage though gradually narrowing exits 40 into the wider space of the successive chambers 43.
  • the multiple successive chambers 34 extend along at least 50% of the total volume of the reactant passage 26, more desirably at least 75% or more, as is the case in the embodiment of Figure 3 .
  • the successive chambers 34 desirably share common walls with the next chambers in the up-and down-stream directions. This helps assure that the maximum number of chambers 34 is positioned within a given space, and thus also maximizes the volume of the reactant passage 26 as a fraction of total volume available between the walls 18, 20.
  • the reactant passage 26 has an open volume of at least 30% of the total volume consisting of (1) said open volume (2) the volume of the wall structures 28 that define and shape the reactant passage between the horizontal walls 18, 20, and (3) any other volume such as empty volume 48 between the wall structures 28 that define and shape the reactant passage 26. More desirably, the reactant passage has open volume of at least 40%.
  • the successive chambers 34 generally desirably do not share common walls with other such chambers not immediately up or downstream, as is such case thermal cross-talk may more easily take place between chambers 34 that are widely separated along the path of the reactant passage 26. Such cross talk can affect the performance of thermally sensitive reactions. Empty volume 48 thus serves to reduce the likelihood of any significant thermal cross talk.
  • corresponding passages 30 of prior art devices such as the device of Figure 2 .
  • the reactant passage 26 divides or forks into two passages twice, first at location F1, and second at locations F2. This counterbalances the decrease of the driving force of the chemical process by locally increasing the residence time. Additionally, the pressure drop within the latter stages of the device decreases correspondingly.
  • Figure 4 is a graph of measured overall heat transfer coefficient in watts per meter-squared and Kelvin as a function of flow rate in milliliters per minute, comparing the embodiment of the present invention represented in Figure 3 . with data points shown as open triangles, to the prior art device of Figure 2 , with data points shown as filled circles.
  • the secondary flows produced by the structures shown in Figure 3 produce a heat transfer advantage of about 50 to 100 W/m 2 K at all flow rates tested. Both of the tested devices were of the same general dimensions and capacities, with a total internal volume of the reactant passage in each case of 5.6 ⁇ 0.1 milliliter.
  • Figure 5 is a graph of percentage mixing performance of a test reaction in a micromixer device as a function of flow rate in milliliters per minute, comparing the embodiment of the present invention described in connection with Figure 3 above to the prior art device described in connection with Figure 2 .
  • the testing method is similar to that of Villermaux J., et al. "Use of Parallel Competing Reactions to Characterize Micro Mixing Effieiency," AlChE Symp. Ser. 88 (1991) 6, p. 286 .
  • the process was to prepare, at room temperature, a solution of acid chloride and a solution of potassium acetate mixed with KI (Potassium iodide).
  • Both of these fluids or reactants were then continuously injected by means of a syringe pump or peristaltic pump into the micromixer or microreactor to be tested.
  • the resulting test reaction involves two competing reactions of different speeds-a "fast” reaction that produces a UV-absorbing end product, and an "ultrafast” one that dominates under ultrafast mixing conditions, producing a transparent solution. Mixing performance is thus correlated to UV transmission, with theoretically perfect or 100% fast mixing yielding 100% UV transmission in the resulting product.
  • the graph of Figure 5 accordingly shows the resulting percentage transmittance as a function of total reactants flow rate.
  • Trace 50 corresponds to the mixing performance of the embodiment of the present invention corresponding to Figure 3
  • trace 52 corresponds to the performance of the prior art device corresponding to Figure 2 .
  • the mixing performance of the embodiment of the present invention is superior, especially at higher flow rates. This is the case even though the embodiment of the present invention of Figure 3 tested also produces less pressure drop than the reference prior art device of Figure 2 . This again shows the achievement of increased process intensification relative to the device of Figure 2 .
  • Figures 7 and 8 dramatically show the comparative advantage of the devices according to the present invention in maintaining dispersions or mixtures of immiscible fluids.
  • Figure 7 shows a portion of digital photograph of a device according to the embodiment of Figure 3 above, tested by being fed equal parts colored water and non-colored heptane at a flow rate for each liquid of 10 milliliters per minute. As shown in the figure, the water and heptane mixture remains well dispersed as it travels from chamber to chamber within this example of a device according to the present invention.
  • Devices according to the present invention have also shown efficiency in dispersing and/or maintaining dispersion of a gas in a liquid.
  • Figure 8 shows a comparative portion of a digital photograph of a prior art device according to Figure 2 above, also being tested with colored water and heptane at 10 milliliters per minute each. As may be seen in the figure, the two immiscible liquid phases coalesce within the passages of the prior art device.
  • Devices according to the present invention can generally create and maintain dispersions or mixtures of immiscible fluids over a wide range of flow rates. Higher flow rates may be used to produce finer dispersions.
  • Figure 9 shows a portion of a digital photograph of a device according to the embodiment of Figure 3 above, with 54 milliliter per minute water flow and 51 milliliter per minute heptane. The light colored granules in the photograph are the small, relatively uniform and wen-dispersed heptane droplets.
  • Figures 10A-10G are cross-sectional plan views of multiple alternative wall structures defining portions of reaction passages according to some alternative embodiments of the present invention, in particular, defining alternative forms of the successive chambers 34.
  • the chambers shown in the embodiments above generally correspond to those of Figure 10F , wherein a post 58 may potentially serve to increase the pressure resistance of the chamber 34 relative to a chamber 34 having a larger open area or "free span" as in the embodiment of Figure 10A .
  • embodiments without the post 58 may have less tendency toward having a small dead volume (a slow moving spot in the fluid flow pattern) upstream of the post 58.
  • the embodiment of Figure 10G essentially avoids all risk of dead volume by including a triangular backing structure 60 on the downstream side of the splitting and re-directing wall 44, being therefore particularly recommended for handling solids such as solid suspensions or precipitating reactions, which can tend to collect in areas of dead volume to clog a reactant passage.
  • the splitting and re-directing wall 44 is segmented in four segments, thus dividing the reactant passage into two main sub-passages around the splitting and re-directing wall 44 and three secondary sub-passages between the segments of the wall 44.
  • the small size of the secondary sub-passages can help to maintain fine emulsions.
  • the splitting and re-directing wall 44 is asymmetrical, being offset to alternating sides in successive chambers 43 so as to provide especially strong secondary flows.
  • the post 58 is also offset from the center of the chamber 43 in alternating fashion, and by being positioned in the larger of the two sub-passages formed by the wall 44, the post 58 serves as an additional flow divider.
  • Figures 10D and 10E correspond to those of 10F and 10B, respectively, with the following difference: the gradually narrowing exit 40 of the previously discussed embodiments is replaced by a wider exit 62 filled with small secondary flow dividers 64 positioned to as to finely divide the incoming flow to the chamber 43, thereby assisting to create and maintain an emulsion or other immiscible mixture.
  • Figure 11 is a cross-sectional plan view of vertical wall structures defining a portion of a reaction passage according to yet another embodiment of the present invention.
  • This embodiment illustrates that the structure of successive chambers 34 utilized in the devices of the present invention may be used in conjunction with other types of mixing devices, such as, in this case, a self-sustaining oscillating mixer chamber 66.
  • Figure 12 shows yet another embodiment of the chambers 34 of the present invention, in which the splitting and re-directing wall 44 is space further from the upstream entrance to the chamber 34 than in some of the previously discussed embodiments.
  • Figure 13 is a cross-sectional plan view of multiple test reaction passages according to various alternative embodiments of the present invention corresponding generally to those shown in Figure 9 , laid out as part of a single device.
  • the mixing test referenced above was performed with each of the test reaction passages 70-82 shown in the figure.
  • test passages 70, 76, and 82 are essentially identical in mixing performance to the device of Figure 2 at 100 milliliters per minute, and are superior at all higher flowrates. This result is further significant in that embodiments without a "mixing zone" as such, including test passages 70 and 76, performed as well as, or better than microfluidic devices having a special mixing section.
  • the chambers of the present invention may be used effectively as mixers as well, without the need for narrow, tortuous passages or other forms of mixer device.
  • Tests were also performed to understand the solids handling capability of the devices of the current invention. Using the following reaction: FeCl3(H2O)6 + 3 NaOH ⁇ Fe(OH)3 + 6H2O + 3 NaCl to form an iron oxide precipitate, the time elapsed until reaching a pressure of 0.7 bar was recorded. A device according to the present invention, including a large number of chambers but not a pre-mixing or other mixing section, was tested in comparison with a device according to Figure 2 above. TABLE II below shows the results: TABLE II Q NaOH (g/min) Q FeCl3 (g/min) Ratio Time to 0.7 bar (sec) Test device 30 11 2.7 394 Comparative 30 11 2.7 25
  • the devices of the type of the present invention were also tested for suitability of Gas/Liquid reactions, by flowing water and nitrogen together at various combinations of flow rates. It was observed that the bubbles of gas remain stable, once created.
  • Specific interfacial area of the gas/liquid dispersion was assessed by a visual method, and is graphed in Figure 15 as a function of gas injection rate on the x axis for water flow rates of 50 milliliters (grey squares) 75 milliliters, (black diamonds) and 100 milliliters per minute. At 100 milliliters per minute, the specific surface area is at least in excess of 12000 m2/m3, with in excess of 14000 m2/m3 available at lower gas flows.
  • Embodiments of devices according to the present invention were also tested for their pressure limits. Results for the device of Figure 3 and comparative results for the device of Figure 2 are summarized in the following table: TABLE III Reactant Passage Thermal Control Passage Test device (five samples) 60.5 bars 26 bars Comparative 52 bars 21 bars
  • microfluidic devices according to the present invention are desirably made from one or more of glass, glass-ceramic, and ceramic. Processes for preparing such devices from glass sheets arming horizontal walls, with molded and consolidated frit positioned between the sheets forming vertical walls, are disclosed, for example, in U.S. Patent No. 7,007,709 , "Microfluidic Device and Manufacture Thereof," but fabrication is not limited to this method.
  • the devices of the present invention may also include layers additional to those shown, if desired.
  • reactant as used herein is shorthand for potentially any substance desirable to use within a microfluidic device.
  • reactant ' and “reactant passage” may refer to inert materials and passages used for such.

Claims (12)

  1. Mikrofluidisches Gerät (10), weiches mindestens einen Reaktionsmitteldurchgang (26) und einen oder mehrere Temperaturregelungsdurchgänge, die in ihm definiert sind, umfaßt, wobei der eine oder die mehreren Temperaturregelungsdurchgänge innerhalb von zwei Volumina (12, 14) positioniert und angeordnet sind, die jeweils von einer Wand (18, 20) begrenzt sind, wobei die Wände (18, 20) im allgemeinen eben und zueinander parallel sind, wobei der Reaktionsmitteldurchgang (26) zwischen den im allgemeinen ebenen Wänden (18, 20) positioniert und durch die im allgemeinen ebenen Wänden (18, 20) und Wände (28), die sich zwischen den im allgemeinen ebenen Wänden (18, 20) erstrecken, definiert ist, dadurch gekennzeichnet, daß:
    - der Reaktionsmitteldurchgang (26) mehrere aufeinanderfolgende Kammern (34) umfaßt, wobei jede solche Kammer (34) eine Aufspaltung des Reaktionsmitteldurchgangs (26) in mindestens zwei Teildurchgänge (36) und eine Vereinigung der aufgespaltenen Durchgänge (36) und eine Änderung der Durchgangsrichtung mindestens eines der Teildurchgänge (36) um mindestens 90 Grad aufweist,
    - jede der mehreren aufeinanderfolgenden Kammern (34), auf welche unmittelbar eine weitere der Kammern (34) folgt, ferner einen sich allmählich verengenden Ausgang (40), welcher einen entsprechenden verengten Eingang (42) der darauffolgenden Kammer (34) bildet, und eine aufteilende und richtungsändernde Wand (44), die quer zu dem unmittelbar stromaufwärts befindlichen Durchgang ausgerichtet und unmittelbar stromabwärts des Eingangs (42) der Kammer positioniert ist, umfaßt, wobei die stromaufwärtige Seite der aufteilenden und richtungsändernden Wand (44) eine konkave Fläche (46) aufweist.
  2. Mikrofluidisches Gerät (10) nach Anspruch 1, dadurch gekennzeichnet, daß die Änderung der Durchgangsrichtung größer als 90 Grad ist.
  3. Mikrofluidisches Gerät (13) nach einem der Ansprüche 1 und 2, dadurch das die Änderung der Durchgangsrichtung eine Änderung der Durchgangsrichtung von mindestens zwei der Teildurchgänge (36) ist.
  4. Mikrofluidisches Gerät (10) nach einem der Ansprüche 1-3, dadurch gekennzeichnet, daß der Reaktionsmitteldurchgang (26) eine konstante Höhe in einer Richtung aufweist, die zu den im allgemeinen ebenen Wänden (18, 20) senkrecht ist.
  5. Mikrofluidisches Gerät (10) nach einem der Ansprüche 1-4, dadurch gekennzeichnet, daß der Reaktionsmitteldurchgang (26) ein offenes Volumen von mindestens 30 % des Gesamtvolumens aufweist, welches aus (1) diesem offenen Volumen, (2) dem Volumen der Wände (28), die sich zwischen den im Allgemeinen ebenen Wänden (18, 20) erstrecken, und (3) jedwedem sonstigen Volumen zwischen den Wänden (28), die sich zwischen den im Allgemeinen ebenen Wänden (18, 20) erstrecken, besteht.
  6. Mikrofluidisches Gerät (10) nach einem der Ansprüche 1-4, dadurch gekennzeichnet, daß der Reaktionsmitteldurchgang (26) ein offenes Volumen von mindestens 40 % des Gesamtvolumens aufweist, welches aus (1) diesem offenen Volumen, (2) dem Volumen der Wände (28), die sich zwischen den im Allgemeinen ebenen Wänden (18, 20) erstrecken, und (3) jedwedem sonstigen Volumen zwischen den Wänden (28), die sich zwischen den im Allgemeinen ebenen Wänden (18, 20) erstrecken, besteht.
  7. Mikrofluidisches Gerät (10) nach einem der Ansprüche 1-6, dadurch gekennzeichnet, daß die zwei oder mehr Teildurchgänge (36) mindestens zwei primäre und einen oder mehrere sekundäre Teildurchgänge enthalten.
  8. Mikrofluidisches Gerät (10) nach einem der Ansprüche 1-7, dadurch gekennzeichnet, daß das Gerät (10) aus einem oder mehreren von Glas, Glaskeramik und Keramik ausgebildet ist.
  9. Mikrofluidisches Gerät (10) nach einem der Ansprüche 1-8, dadurch gekennzeichnet, daß sich die mehreren aufeinanderfolgenden Kammern (34) entlang von mindestens 30 % des Volumens des Reaktionsmitteldurchgangs (26) erstrecken.
  10. Mikrofluidisches Gerät (10) nach einem der Ansprüche 1-8, dadurch gekennzeichnet, daß sich die mehreren aufeinanderfolgenden Kammern (34) entlang von mindestens 50 % des Volumens des Reaktionsmitteldurchgangs (26) erstrecken.
  11. Mikrofluidisches Gerät (10) nach einem der Ansprüche 1-8, dadurch gekennzeichnet, daß sich die mehreren aufeinanderfolgenden Kammern (34) entlang von mindestens 75 % des Volumens des Reaktionsmitteldurchgangs (26) erstrecken.
  12. Mikrofluidisches Gerät (10) nach einem der Ansprüche 1-11, dadurch gekennzeichnet, daß sich der Reaktionsmitteldurchgang (26) einmal oder mehrere Male in mindestens zwei Zweige gabelt (F1, F2).
EP07301225A 2007-07-11 2007-07-11 Mikrofluidische Geräte für verstärkte Verfahren Active EP2017000B1 (de)

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EP07301225A EP2017000B1 (de) 2007-07-11 2007-07-11 Mikrofluidische Geräte für verstärkte Verfahren
US12/171,403 US7939033B2 (en) 2007-07-11 2008-07-11 Process intensified microfluidic devices
KR1020107003067A KR101666635B1 (ko) 2007-07-11 2008-07-11 공정 강화된 미세유체 장치
MX2010000485A MX2010000485A (es) 2007-07-11 2008-07-11 Dispositivos microfluidicos de proceso intesificado.
CN2008801070305A CN101873890B (zh) 2007-07-11 2008-07-11 过程加强的微流体装置
AU2008275602A AU2008275602A1 (en) 2007-07-11 2008-07-11 Process intensified microfluidic devices
JP2010516065A JP2011508657A (ja) 2007-07-11 2008-07-11 プロセス強化マイクロ流体装置
RU2010104674/05A RU2010104674A (ru) 2007-07-11 2008-07-11 Микроструйные устройства с интенсификацией процесса
TW097126566A TWI363656B (en) 2007-07-11 2008-07-11 Process intensified microfluidic devices
CA2693463A CA2693463A1 (en) 2007-07-11 2008-07-11 Process intensified microfluidic devices
PCT/US2008/008535 WO2009009129A1 (en) 2007-07-11 2008-07-11 Process intensified microfluidic devices
BRPI0813700-5A2A BRPI0813700A2 (pt) 2007-07-11 2008-07-11 Dispositivos microfluidos com intensificação de processos
ZA201000944A ZA201000944B (en) 2007-07-11 2010-02-09 Process intensified microfluidic devices
JP2014056426A JP6204235B2 (ja) 2007-07-11 2014-03-19 プロセス強化マイクロ流体装置
JP2017166629A JP6674933B2 (ja) 2007-07-11 2017-08-31 プロセス強化マイクロ流体装置
JP2020039661A JP7049381B2 (ja) 2007-07-11 2020-03-09 プロセス強化マイクロ流体装置

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US20090028763A1 (en) 2009-01-29
CA2693463A1 (en) 2009-01-15
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JP2020114585A (ja) 2020-07-30
JP6204235B2 (ja) 2017-09-27
CN101873890A (zh) 2010-10-27
MX2010000485A (es) 2016-01-27
JP2018051553A (ja) 2018-04-05
RU2010104674A (ru) 2011-08-20
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TWI363656B (en) 2012-05-11
JP7049381B2 (ja) 2022-04-06
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EP2017000A1 (de) 2009-01-21
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JP2011508657A (ja) 2011-03-17

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